CN104525234A - Preparation method for graphite-phase carbon nitride photocatalytic material - Google Patents
Preparation method for graphite-phase carbon nitride photocatalytic material Download PDFInfo
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Abstract
The invention discloses a preparation method for a polymorphic multi-scale multidimensional graphite-phase carbon nitride photocatalytic material, belonging to the technical field of functional materials. The preparation method comprises the following steps: 1) selecting a biomass material as a template, and pre-treating the template; 2) further performing soaking treatment of a TEOS solution and a water-bath thermal insulation treatment on the template; 3) roasting the template within a temperature range of 550 DEG C-650 DEG C under a non-oxidative inert atmosphere; 4) soaking the template into a cyanamide solution, preserving the heat for 2-4 hours at 50-60 DEG C, raising the temperature to 550 DEG C-600 DEG C at a temperature rise rate of 1-2.5 DEG C/minute in the presence of argon gas and preserving the heat for 3-7 hours; 5) adding the template into a 4-6 mol/L NH4HF2 solution to stand for 48-52 hours, and drying under a vacuum condition at 60-65 DEG C after cleaning with alcohol and water. The photocatalytic graphite-phase carbon nitride material prepared by the preparation method disclosed by the invention has the characteristics of low cost and a wide source, relatively high light absorption capacity, and can be used for overcoming the defects that the luminous reflectance is low, the absorption rate is low and the efficiency in the whole catalytic process is low.
Description
Technical field
The present invention relates to a kind of preparation method of graphite phase carbon nitride, particularly a kind of preparation method utilizing biological template to prepare the multiple dimensioned graphite phase carbon nitride catalysis material of polymorphic various dimensions, belong to material preparation and photocatalysis field.
Background technology
Graphite phase carbon nitride is a kind of catalysis material in the past few years risen, there is unique electronic structure and excellent chemical stability, in recent years not only by as the catalyst of not metallic components and catalyst carrier, be widely used in the load of the noble metals such as the selective conversion of organo-functional group, photochemical catalyzing, hydrogen reduction and Au, Pd, Ag, Pt, be also used for H by as green energy-storing material and hard mould agent
2, the storage of CO and the preparation etc. of nano metal nitrogen (oxygen) compound, cause the concern of people gradually at the energy and material association area.
Find, around the preparation method of graphite phase carbon nitride catalysis material, have many bibliographical informations by literature search.As Chinese patent application CN201410089569.X, name is called: " a kind of graphite phase carbon nitride hollow ball visible light catalyst of combined polymerization modification ", the technical characterstic of this patent is with mesoporous silica spheres as template, using cyanamide and organic molecule monomer as predecessor, obtain graphite phase carbon nitride hollow ball by thermal polymerization and removal template, the method has the simple advantage of synthesis technique, but particle diameter is single, there is no variform and yardstick, be of limited application.Chinese patent application CN201410038958.X for another example, name is called " ionic liquid promotes synthetic graphite phase carbon nitride nanometer sheet visible light catalyst ", the technical characterstic of this patent is for presoma with urea and dialkylimidazolium tetrafluoro boric acid ionic liquid at room temperature, formed by high temperature instrument and effect, the method can synthesize low-dimensional nanoscale twins microstructure, but form is single, synthesis technique is complicated, does not have the change of multiple yardstick.
Summary of the invention
The present invention is directed to shortcomings and deficiencies of the prior art, thering is provided a kind of take living beings as the method for the polymorphic multiple dimensioned multidimensional number graphite phase carbon nitride catalysis material of Template preparation, preparation technology is relatively simple, the catalysis material prepared is widely used, have the advantages that form of diverse, catalytic efficiency are high, can adapt to the reaction of different dimensions different phase, and efficiently solve catalysis material complicated process of preparation in the past, the drawback that the scope of application is little.
The present invention by adopt biological material that is with low cost, wide material sources be raw material, through cleaning, drying, then through the dipping of precursor in living beings structure, assemble and fire, namely obtain a kind of photocatalysis graphite phase carbon nitride material of superior performance.
Technical scheme of the present invention is as follows:
A preparation method for graphite phase carbon nitride catalysis material, method step is mainly as follows:
1) choose biological material such as fresh bio material, carry out pre-treatment, pre-treatment specifically refer to by described biological material ethanol and distillation underwater cleaning, in NaOH solution, soak 2-4h afterwards;
Some concrete examples of pretreatment process can be: for butterfly's wing, soak 10min in ethanol, taking-up is put in water and is cleaned 3-4 time, is put in the solution mixed by 4g NaOH and 200ml distilled water and soaks 2h, again put in distilled water and clean 3-4 time; For rape pollen, through ethanol purge 2 times, distilled water cleans 5 times; Then be dipped among NaOH weak solution, 50 DEG C of water bath heat preservation 8h;
2) ethyl orthosilicate TEOS solution is provided, as provided by obtain solution; The biological material that pre-treatment is good is put into TEOS solution, water bath heat preservation a period of time, wherein the temperature of water bath heat preservation is 50 DEG C-55 DEG C, and temperature retention time is 6-10h.
The formula of TEOS solution can be: the TEOS of 6-10g adds among 180ml ethanol, adds HCl and the 20-30ml distilled water that 3ml mass fraction is 37% after stirring, and stirs as 1h;
3) by through step 2) template that processes calcines; Calcination process programming rate is 1-2 DEG C/min, and calcining heat is 550-650 DEG C, and calcination time is 10-12h;
4) template that step 3) is handled well is added in cyanamide solution be incubated a period of time, calcine under argon atmosphere after cleaning, drying;
Described cyanamide solution is preferably 4-8g cyanamide, adds 150ml distilled water gained; Described holding temperature is 50 DEG C-60 DEG C, and temperature retention time is 2h-4h; Described calcination condition is that the programming rate of 1-2.5 DEG C/min is heated to 550 DEG C-600 DEG C and is incubated 3-7h;
5) take out 4) in template be generally Powdered template and add NH
4hF
2soak in solution, after cleaning, drying can obtain graphite phase carbon nitride catalysis material;
Described NH
4hF
2the concentration of solution is 4-6mol/L, and soak time is 48h-52h, and baking temperature is 60 DEG C-65 DEG C.
Described biological material, can be selected from least one of the biological material of one dimension form, Two-dimensional morphology or three-dimensional configuration; Wherein, the biological material template of one dimension form has bar-shaped virus, bacterium, unicellular microorganism etc.; The biological material template of Two-dimensional morphology has petal, refers in particular to camellia, one towards light violet stem, Gordonia Acuminata slide plate; Three-dimensional biological material template has butterfly's wing, pollen, leaf, egg film, wood, and wherein butterfly refers to the one in skirt swallowtail butterfly, control of Papilio paris, green secondary rainbow moral swallowtail butterfly; Pollen refers to the one of rape pollen, matrimony vine pollen, astragalus farina, sophora flower pollen; Leaf refers to a kind of blade in flowering cherry, camphor tree, oleander or maple blade; Wood refers to the one in white pine, peach, willow; Egg film refers to the one in eggshell membrane, membrane of duck egg, goose egg film.
Compared with prior art, beneficial effect of the present invention is as follows:
The catalysis material that the present invention obtains can contain one dimension to three-dimensional structural form, and with low cost, the feature such as technique is relatively simple, has specific area large, and the avtive spot of unit are is many; Catalysis material prepared by simultaneously the present invention also has the structure effect strengthening light absorption, efficiently solves the catalysis material in the past prepared very large and cause the drawback that most of luminous energy is not used effectively for the reflection of light.
Graphite phase carbon nitride material prepared by the present invention can be applied to the photocatalysis Decomposition of pollutant, the photocatalysis synthesis of organic material, at electronics, electrically, there is good application prospect in communication, the field such as national defence, drive or pollution plot class industry as can be applicable to all kinds of photoelectricity, greatly can improve the efficiency of reaction, reduce reaction cost.
Certainly, implement arbitrary product of the present invention might not need to reach above-described all advantages simultaneously.
Detailed description of the invention
The invention provides a kind of preparation method of graphite phase carbon nitride catalysis material, it comprises the steps:
1) select biological material as template, and described biological material is carried out pre-treatment, described pre-treatment comprises takes out drying by described template at ethanol and distillation underwater cleaning, soaks 2-4h afterwards in NaOH solution; Described biological material be selected from the biological material of the biological material of one dimension form, the biological material of Two-dimensional morphology and three-dimensional configuration at least one of them;
2) more further under non-oxygen inert atmosphere through step 2) template that processes to immerse in TEOS solution and water bath heat preservation process in 50-55 DEG C of temperature range, temperature retention time 6-10h;
3) will through step 2) template that processes with the calcining of the programming rate of 1-2 DEG C/min, calcining heat 550 DEG C-650 DEG C, calcination time 10-12h;
4) then add in cyanamide solution by the template of above-mentioned process, holding temperature is 50 DEG C-60 DEG C, and the time is 2-4h, calcines afterwards in argon atmosphere, with the programming rate to 550 of 1-2.5 DEG C/min DEG C-600 DEG C, and calcining 3-7h;
5) product of step 4) is added in NH4HF2 solution, leave standstill 48-52h, finally in temperature 60 C-65 DEG C of dryings, obtain graphite phase carbon nitride catalysis material with ethanol purge.
In this article, the scope represented by " numerical value is to another numerical value " is a kind of summary representation avoiding all numerical value enumerated in the description in this scope.Therefore, the record of a certain special value scope, the comparatively fractional value scope containing any number in this number range and defined by any number in this number range, as expressly write out this any number in the description, comparatively fractional value scope is the same with this.
Below in conjunction with specific embodiment, set forth the present invention further.Should be appreciated that, these embodiments only for illustration of the present invention, and are not intended to limit the scope of the invention.The improvement made according to the present invention of those skilled in the art and adjustment, still belong to protection scope of the present invention in actual applications.
Embodiment 1
Virus or the bacterium of choosing one dimension are raw material, through ethanol purge 3 times, then flood in NaOH solution after 1 hour, take out dry.Will process dried viral powder is incubated 6h after fully mixing with the TEOS solution prepared in 50 DEG C of water-baths, and further under non-oxygen inert atmosphere, be warming up to 550 DEG C with the speed of 1 DEG C/min, be incubated 12h.Then put into cyanamide solution, the lower 50 DEG C of insulation 2h of vacuum condition, are heated to 550 DEG C of insulation 4h with the programming rate of 2.3 DEG C/min, then put into the NH of 4mol/L under non-oxygen inert atmosphere
4hF
2in solution, soak 48h, after ethanol and distilled water cleaning, dry and can obtain the one dimension catalysis material with good light absorption and catalytic performance.
Embodiment two
Choose camellia petal, through ethanol purge 3 times, then flood in NaOH solution after 1 hour, take out dry.Will process dried camellia petal is incubated 6h after fully mixing with the TEOS solution prepared in 50 DEG C of water-baths, and further under non-oxygen inert atmosphere, be warming up to 650 DEG C with the speed of 1.5 DEG C/minute, be incubated 10h.Then put into cyanamide solution, the lower 70 DEG C of insulation 2-3h of vacuum condition, are heated to 550 DEG C of insulation 2h with the programming rate of 2.3 DEG C/min, then put into the NH of 4mol/L under non-oxygen inert atmosphere
4hF
2in the aqueous solution, soak 48h, the post-drying through ethanol and distilled water cleaning can obtain the two-dimentional catalysis material with good light absorption and catalytic performance.
Embodiment three
Choosing butterfly's wing is raw material, uses soaked in absolute ethyl alcohol 10min, then floods in NaOH solution after 1 hour, takes out dry.Will process dried rape pollen is incubated 6h after fully mixing with the TEOS solution prepared in 50 DEG C of water-baths, and further under non-oxygen inert atmosphere, be warming up to 650 DEG C with the speed of 1.5 DEG C/minute, be incubated 10h.Then put into cyanamide solution, the lower 70 DEG C of insulation 2-3h of vacuum condition, are heated to 550 DEG C of insulation 4h with the programming rate of 2.3 DEG C/min, then put into the NH of 4mol/L under non-oxygen inert atmosphere
4hF
2in the aqueous solution, soak 48h, the post-drying through ethanol and distilled water cleaning can obtain the three-dimensional light catalysis material with good light absorption and catalytic performance.
Embodiment four
Choose the intact homogeneous leaf of form as material, through ethanol purge 3 times, then flood in NaOH solution after 1 hour, take out dry.Will process dried rape pollen is incubated 6h after fully mixing with the TEOS solution prepared in 50 DEG C of water-baths, and further under non-oxygen inert atmosphere, be warming up to 600 DEG C with the speed of 1.5 DEG C/minute, be incubated 12h.Then put into cyanamide solution, the lower 70 DEG C of insulation 2-3h of vacuum condition, are heated to 550 DEG C of insulation 4h with the programming rate of 2.3 DEG C/min, then put into the NH of 4mol/L under non-oxygen inert atmosphere
4hF
2in water-soluble, soak 48h, the post-drying through ethanol and distilled water cleaning can obtain the three-dimensional light catalysis material with good light absorption and catalytic performance.
Embodiment five
Choose rice husk as raw material, through ethanol purge 3 times, then flood in NaOH solution after 1 hour, take out dry.Will process dried rape pollen is incubated 6h after fully mixing with the TEOS solution prepared in 50 DEG C of water-baths, and further under non-oxygen inert atmosphere, be warming up to 650 DEG C with the speed of 1.5 DEG C/minute, be incubated 10h.Then put into cyanamide solution, the lower 70 DEG C of insulation 2-3h of vacuum condition, are heated to 550 DEG C of insulation 4h with the programming rate of 2.3 DEG C/min, then put into the NH of 4mol/L under non-oxygen inert atmosphere
4hF
2in the aqueous solution, soak 48h, the post-drying through ethanol and distilled water cleaning can obtain the three-dimensional light catalysis material with good light absorption and catalytic performance.
Photocatalysis graphite phase carbon nitride material prepared by the present invention has feature that is with low cost, wide material sources on the one hand, and have higher light absorpting ability on the other hand, overcome light reflectivity high, absorptivity is low, the inefficient drawback of whole catalytic process.
Under the instruction of the present invention and above-described embodiment, those skilled in the art are easy to predict, cited or each raw material that exemplifies of the present invention or its equivalent alterations, each processing method or its equivalent alterations can realize the present invention, and the parameter bound value of each raw material and processing method, interval value can realize the present invention, do not enumerate embodiment at this.
Claims (8)
1. a preparation method for graphite phase carbon nitride catalysis material, is characterized in that, comprises the steps:
1) select biological material as template, and described biological material is carried out pre-treatment, described pre-treatment comprises takes out drying by described template at ethanol and distillation underwater cleaning, soaks 2-4h afterwards in NaOH solution; Described biological material be selected from the biological material of the biological material of one dimension form, the biological material of Two-dimensional morphology and three-dimensional configuration at least one of them;
2) more further under non-oxygen inert atmosphere through step 2) template that processes to immerse in TEOS solution and water bath heat preservation process in 50-55 DEG C of temperature range, temperature retention time 6-10h;
3) will through step 2) template that processes with the calcining of the programming rate of 1-2 DEG C/min, calcining heat 550 DEG C-650 DEG C, calcination time 10-12h;
4) then add in cyanamide solution by the template of above-mentioned process, holding temperature is 50 DEG C-60 DEG C, and the time is 2-4h, then calcines in argon atmosphere, with the programming rate to 550 of 1-2.5 DEG C/min DEG C-600 DEG C, and calcining 3-7h;
5) product of step 4) is added NH
4hF
2in solution, leave standstill 48-52h, finally in temperature 60 C-65 DEG C of dryings, obtain graphite phase carbon nitride catalysis material with ethanol purge.
2. the preparation method of graphite phase carbon nitride catalysis material according to claim 1, is characterized in that, the biological material of described one dimension form is selected from bar-shaped virus, bacterium or unicellular microorganism; The biological material of described Two-dimensional morphology is selected from petal; The biological material of described three-dimensional is selected from the one of butterfly's wing, pollen, leaf, egg film or wood.
3. the preparation method of graphite phase carbon nitride catalysis material according to claim 2, is characterized in that, described petal is selected from camellia, one towards light violet stem or Gordonia Acuminata petal.
4. the preparation method of graphite phase carbon nitride catalysis material according to claim 2, is characterized in that, described butterfly is selected from the one in skirt swallowtail butterfly, control of Papilio paris, green secondary rainbow moral swallowtail butterfly; Described pollen is selected from the one of rape pollen, matrimony vine pollen, astragalus farina, sophora flower pollen; Described leaf is selected from a kind of blade in flowering cherry, camphor tree, oleander or maple; Described wood is selected from the one in white pine, peach, willow; Described egg film is selected from the one in eggshell membrane, membrane of duck egg, goose egg film.
5. the preparation method of graphite phase carbon nitride catalysis material according to claim 1, is characterized in that, in described step 1), soaks biological material with the NaOH that volumetric concentration is 1.8-2.5%.
6. the preparation method of graphite phase carbon nitride catalysis material according to claim 1, it is characterized in that, step 2) described in TEOS solution refer to: the TEOS of 6-10g adds among 180ml ethanol, adds the mixed solution that HCl and 20-30ml distilled water that 3ml mass fraction is 37% obtains after stirring.
7. the preparation method of graphite phase carbon nitride catalysis material according to claim 1, is characterized in that, the cyanamide solution described in step 4) refers to that 4-8g cyanamide adds the solution of 150ml distilled water gained.
8. the preparation method of graphite phase carbon nitride catalysis material according to claim 1, is characterized in that, the NH described in step 5)
4hF
2solution refers to that molar concentration is the NH of 4-6mol/L
4hF
2solution.
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| CN105413731A (en) * | 2015-12-14 | 2016-03-23 | 华南理工大学 | Carbon-doped nano-catalyst as well as preparation method and application thereof |
| CN105879894A (en) * | 2016-04-25 | 2016-08-24 | 陕西科技大学 | (NH4)2SiF6/mpg-C3N4 powder and preparation method and application thereof |
| CN111389448A (en) * | 2020-05-06 | 2020-07-10 | 西南科技大学 | Graded porous g-C for photocatalytic degradation3N4Preparation method of @ wood composite material |
| CN113210012A (en) * | 2021-04-23 | 2021-08-06 | 江苏科技大学 | Artificial single cell structure material and preparation method and application thereof |
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